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" Patented Jan. 15, 1929.

UNITED STATES,

. eeazza PATENT OFFICE.

1 WILLIAM 1 news, or crwrrmm, rinw .rnn i MARY GARDNER DOWNS ADMINIS- mm or sun WILLIAM'F. nowNs, nncnasnn.

"-ZPMGESB FOB MANUFACTURE OE .ANHYDROUS METALLIC CHLORIDEQ.

Io Drawing.

Metallic chlorides are almost universally soluble in water, the notable exception being silver chloride. Practically all metallic 10 chlorides can be volatilized and condensed as stable compounds.

Anhydrous aluminum chloride can not be so produced because when theattempt is -made to-drive the water from its hydrous 1 form by the application of heat, it breaks V up into alumina as a residue and the chlorine passes off with the water mainly as hydro; chloric acid fumes.

- So e other chlorides such for example as' selenium and titanium possess the same prop- 'erties, and all such can be made by the process herein described and the rocess is especially useful for the manu acture of anhydrous aluminum chloride which is now 95 so much desired.

Much trouble is disclosed by the various inventions as to the difiiculty of finding proper and durable materials to be used in the construction of the apparatus in which the materials are brought into contact.

At the temperature necessary, chlorine has a corrosive action on most of the materials that can be obtained for said apparatus. Fused silica is hi hly resistant to this action and now can go obtained in various grades of purity and shapes which are available for the purpose.

The higher the percentage of the silica in such compositions the more resistant they are to the corrosive action of hot chlorine.

It is not the purpose here to discuss or claim special materials for the manufacture of an apparatus in which to make anhydrous metallic chlorides, but to set forth the particular novel method of so producing physical adherent contact of minute particles of carbon and a metallic oxide that, when hot chlorine is passed through and over such adherent particles, all three of the necessary ingredients are simultaneously within the same sphere of reactive influence and the desired chloride: is efiiciently produced thereby.

It is generally well known that under the rially rides, thus making it lmpra'ctical commerci- I Application filed 1121111913712, 1925. Serial No. 1,935.

conditions of temperature employed, chlo-;

rine and carbon do not react on one another; it is also well known that chlorine does not react; on aluminaunder similar conditions; and also carbon andalumina do not react on each other under like conditions.

. Thereaction demands that all three (3). ingredients must be simultaneously within' the sphere of reactive influence.

If carbon has been previously combine with chlorine as carbon tetra-chloride then this combination. may be made to act as an,

integral unit and the contact of this unit with alumina gives the desiredsimultaneous contact of all three ingredients.

This would mean that carbon tetrachloride would be the reactive agent to be used.

The fact that carbon tetra-chloride can be used in the manufacture of anct-allic chlorides is not disputed, but its use adds mate to the cost of making metallic chloally.

A similar explanation would apply to the use of aluminum carbide and chlorine for the manufacture of aluminum chlorides.

The difiiculties and cost of making aluminum carbide precludes its consideration altogether.

Carbon, alumina and free chlorine constitute b far the cheapest groupof raw materials t at can be used in the manufacture of aluminum chloride.

The use of the oxide of many other metals would likewise constitute the cheapest group of raw.materials designed to make their particular chlorides.

The particular purposeof this invention is to so contact the two solids, carbon and metallic oxide, that they remain in adherent contact throughout all the physical changes and movement incident to their being brou ht into contact with the hot chlorine.

In order to bring about this adherent contact I use some organic substance which calcined or lasses will be full -;ratio of fifteen parts of carbon to eighty-five (85) part alumina, as has been shown to be the required ratio'in the formula'alread discussed.

I also ta e care that the volume of the solutitin used is fully suiiicient to completely wet aijd intimately mix with the quantity of alumina used. If the particular organic substance used isja thin liquid but little or no solvent will be required. T he volume of the solution oforganic substance must always be sufiicientto fully wet and intimately mix with the particles of metallic oxide-being used. ,Arnexcess of sovent or volume of oranic solution simply requires longer time or evaporation. Part of the required amount of carbon may be added as such'. I prefer, however, that the full com lement of carbon required is obtained from t e organic substance used.

' To make this more specific I give the following figures, black strap molasses yields an average of thirty (30) psi cent residual ficarbon, this means that fifty pounds of black stra molasses would yield fifteen (15) pounds of residual carbon.

' Therefore, in carrying out my process, to

fift (50) ounds or such mo asses I add g'h ty-five 85) poundsof'alumina together with sutiicient water so that the volume of 'thesolution thoroughly wets and intimately miifics with the fine particles of the alumina use The. finer the alumina the greater the volume of solution required,

After thoroughl commingling-this mixture I evaporate t 0 solution until a pasty mass somewhat like a caramel mixture is obtained.

The temperature is thenraised and air excluded until the mass .is charred.

This may be done in the.same vessel, or thepasty, caramel like massmay be transferred to some other vessel according to the conveniences of the e'quipmentat hand.

The charred mass is cooled to a temperature below that-ofwxidation of carbon before exposure air.

Itwxll be found to be porous and easily :crushed to fine particles'as desired.

Each particle of alumina will .be found to have its due proportion of adherent carbon; it will also be found that the. adherent contact of the carbon and alumina is sufiiciently strong to hold them to ether throughoutthe physical movements of handling and feeding them' into ,a'- reaction chamber where they are to come in contact with hot chlorine in chloride.

Having in this novel way so contacted the the manufacture of anhydrous aluminum,-

' two solids,- carbon and the'metaliic oxide,-

that they act as an integral unit when subjectedto the. action of hot chlorine, I next feed them into ,1. reaction chamber, and said chamber may be either revolving'or, stationury.

reactionchumber' are that it can be maintained at a regulated temperature by 'ex- So far the process herein (loscribed is concerned the requirements of The feeds of the conamount with reference to one another-as per the ratio of weight requirements shown by the chemical formulae, care being taken that there sh all be always a quantity of the solids present in the reaction chamber in excess of the combining requirements of the amount of chlorine present at any 'moment.

The two feeds have each their own so arate I sources of supply and are so arrange with reference to one another that the feed of chlorine passes through and over the supply gf solids maintained in the reaction cham- As these materials come in contact in the reaction chamber under proper temperature control, the reaction set forth in the chemical equation given occurs and anhydrous metallic chloride is produced. In the illustration given this=is anhydrous aluminum chloride. As the ases evolves from the reaction soon fill t e reaction chamber, an exit for their esc'a e is provided by which they pass to con ensers and the metallic chloride condensed and collected in the usual manner.

I claim v 1. The}, recess of maln'ng an v anhydrous 'metallidh loride which comprises mixin the oxide of the then with a solution 0 residual harbon yielding organic compound of such proportions as give the required ratio of carbon to the oxide used, intimately mixing the oxide in this solution, evaporate.

and feeding these solids in their idhernt ing the solvent, chairing the residuajlmass, m

' metallic. c

mamas contact into a rerolving reaction chamber against a regulated current of hot chlorine, maintaining the temperature of said chamher by external heat and condensihg the metallic chloride from the gases evolved."

2. The process of making aluminum chloride which comprises mixing alumina with a solution of residual carbon fyieldingwrganic compoundof such roportions as give quired ratio of carbon to the oxide used, inti and feeding these" solids give the required contact into a revolvingv charring the residual mass and lated-fcurrent of hot chlorine,

the temperature of said chamber heat and condensing the aluminum chloride 45 I In testimony whereof I afiix mately mixing the oxide in this solution;

evaporating the solvent, chairing the resid-' ual mass, adherent chamber against a regulated currentof hot chlorine, maintaining the temperature of said chamber by external heat and condensing the metallic chloride from they gases evolved.

4. The recess of making aluminum chloride which coin rises mixing alumina with a solution of mo asses in such and feeding these solids in their proportions as ratio of carbon to the alumina used, intimately mixing the alumina in this solution, evaporatin the solvent,

solids in their adherent contact into a re- "volving reaction chamber against a re maintaining by external from the gases evolved.

' ature.

in S1 WILLIAM F. ho NS.

contact into a revolving reactioneeding these 

